CN101260569B - Regenerated cellulose viscose fiber and its preparing process - Google Patents
Regenerated cellulose viscose fiber and its preparing process Download PDFInfo
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Abstract
The invention provides a regenerated cellulose Novamat prepared by stalks of banana as material and a preparation method thereof. The method comprises the following steps of: mechanically knocking the stalks of banana, and performing the devillicate; removing the colloid in the acquired fiber of banana by devillicate through dilute aqueous alkali; mixing the acquired fiber of banana with concentrated aqueous alkali to prepare alkali cellulose; etiolating the acquired alkali cellulose after acid treatment, and dissolving the etiolated alkali cellulose to prepare spinning dope; spinning the acquired spinning dope to acquire the Novamat. The regenerated cellulose Novamat prepared by stalks of banana as material has the characteristics that the Novamat is prepared by cellulose extracted from the stalks of banana as material; the prepared fiber can either be cut staple or long staple with good softness, hydroscopic property and chromaticity, can either be independently manufactured into textile or other blended fibers, thereby creating a new field for the comprehensive use of banana and the development of novel fibers thereof.
Description
Technical field
The present invention relates to produce regenerated cellulose viscose fiber by plant fiber material, a kind of cane with the Musaceae plant of more specifically saying so is that raw material is produced viscose and preparation method thereof.
Background technology
Introducing along with new ideas such as " green, ecological, environmental protection ", under the simultaneously constantly high and severe situation that can the amount of adopting sharply descends in current oil price, the chemical synthetic fiber industry that with the oil is raw material will face raising up significantly of production cost, not have the awkward situation that rice is cooked even.The fiber that the development of new natural material is made has not only overcome the bottleneck of petroleum resources, and has catered to the green weaving trend based on " ecological, fashion is purpose ".Development of new natural fabric resource is the task of top priority.Banana is one of four big fruit in the world, and cultivated area is only second to grape, citrus, occupies the 3rd.Banana originates in the southeast, Asia, and China south China is one of any of several broadleaf plants class cradle.The banana cultural area has spread all over north and south latitude 30 degree with the interior torrid zone, wide area, subtropical zone, has more than 120 countries and regions that banana production is arranged.Banana occupies critical role on international fresh fruit market.At present, province (autonomous region) such as China Hainan, Guangdong, Guangxi, Yunnan and Taiwan are all planted and are implanted with banana.The cultivated area of China's banana in 2004 is 28.5 ten thousand hectares, and 6,290,000 tons of output are in the 5th in the world and the 3rd, nearly 10,000,000,000 yuan of the gross annual output value of banana respectively.Banana occupies very consequence on international fresh fruit market, whole world banana production is only second to Citrus and occupies the 2nd.Stay a large amount of outmoded canes after banana is picked, utilize banana stalk that very big economic worth is arranged.The cane of finding banana after deliberation contains a large amount of cellulose components, has people's research and utilization banana stalk to extract fiber and is used for papermaking and makes paper products, as Chinese patent CN200310105776.1.Because banana fiber is stone, can be the key of technology with the such smooth fine fibre of its fiber treatment imaging cotton fiber.Banana cloth feel such as fiber crops that the upright product of Tokyo, Japan technical research institute is developed into can be used to make the packaging bag of outlet coffee.Fiber (accounting for 30%) and cotton (70%) blending that clear textile company utilization of day is extracted out from the banana stem are made clothings such as overcoat.The said firm represents this research of beginning before 2 years, though it is still under test to use banana fiber to make clothing at present.Banana fiber can be used for making household supplies, and the fiber of hand stripping can be used for producing handbag and other adornments, or processes resultant yarn on the jute spinning equipment, makes rope and gunnysack.(Japan's " fibre science ", 2003 (1): 52; Wang Xiaoji: day the present invention is a kind of to be the packaging bag of raw material with the banana fiber, Guangdong printing, 2005 (3): 5; Qu Cailian etc.: several novel plant fibers and application thereof, the fine inspection of China, 2006 (5): 32～34; ) chemical composition of banana fiber mainly is cellulose, hemicellulose and lignin, in addition, also have a small amount of ash content and the hydrotrope, cellulose 58.5%-76.1% wherein, hemicellulose 28.5-29.9% (in 1% NaOH solution, recording), lignin 4.8%-6.13%, ash content 1.0%-1.4%, hydrotrope 1.9%-2.61%.
At present, viscose is to be raw material with native celluloses such as timber, cotton linters, a kind of broad-spectrum regenerated celulose fibre that makes through a series of processing procedures such as boiling, acid treatment, bleaching.Because this fiber and fabric thereof have good suction, moisture resistance, and be soft, comfortable and easy to wear,, be subjected to consumers in general's favor deeply near natural woolliness.Particularly back to nature, green consumption is current, the fabric demand that with the natural fabric is raw material grows with each passing day especially, but worsening shortages along with traditional raw materials such as timber, cotton linters, production cost sharply rises, therefore, it is imperative that new raw material is explored in exploitation, simultaneously, from health, health care equal angles, also more characteristic requirement is proposed textile raw material.At present since directly performance such as the fiber feel of extracting from banana stalk and synthetic fiber also show slightly poor, mostly make some technology textiless.
Summary of the invention
The object of the present invention is to provide a kind of cane with the Musaceae plant is the regenerated cellulose viscose fiber of feedstock production.
Another object of the present invention is to provide a kind of cane with the Musaceae plant is the method for feedstock production regenerated cellulose viscose fiber.
A kind of regenerated cellulose viscose fiber comprises viscose filament yarn and viscose staple fibre, it is characterized in that described viscose filament yarn and viscose staple fibre all are that stem stalk with the Musaceae plant is that feedstock production obtains; The fineness of described viscose filament yarn and viscose staple fibre is 2.2-2.7dtex, and dried fracture strength is 2.3-2.9CN/dtex, wet breaking strength Wei ≧ 1.10CN/dtex, dried elongation at break Wei ≧ 16%.
The preparation method of above-mentioned viscose may further comprise the steps:
(1) the stem stalk of Musaceae plant is carried out machinery and knock, carry out the branch silk then, obtain the Musaceae string;
(2) will divide the colloid in the Musaceae string that obtains to remove with dilute alkaline soln, after washing, obtain the Musaceae plant cellulose again;
(3) resulting Musaceae string is mixed with concentrated alkali solution produce alkali cellulose;
(4) alkali cellulose with gained carries out yellow after acid treatment, then its dissolving is made spinning slurry;
(5) spinning slurry with gained carries out spinning, obtains viscose.
Described step (1) is carried out the process that machinery also comprises that the cane with the Musaceae plant sorts, cuts off before knocking to the cane of Musaceae plant.
Describedly will divide the colloid in the Musaceae string that obtains of silk to remove with dilute alkaline soln, obtaining Musaceae plant cellulose concrete grammar again after washing drying is: the fiber that divides silk to obtain, putting into NaOH is that the aqueous slkali of 0.8-1.5% boiled 2-3 hour to the over dry raw material, liquor ratio is: 1:4-1:10 gets the banana fiber element after washing, drying.
The described method that resulting Musaceae plant cellulose and concentrated alkali solution are mixed with alkali cellulose is: it is 18--23 ℃ that Musaceae plant haulm cellulose is immersed temperature, concentration is in the aqueous solution of NaOH of 240-250 grams per liters, flood after 60-120 minutes, take out alkali cellulose, after squeezing unnecessary alkali lye, the weight percentage of alkali cellulose is 30-33% in the band liquid caustic soda cellulose.
Describedly with alkali cellulose yellow, the method for preparing spinning slurry be: with above-mentioned alkali cellulose and weight is that the carbon disulfide of alkali cellulose 25-35% reacts, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, reaction time 40-70 minute, make cellulose xanthate, the cellulose xanthate that makes is cooled to 10-14 ℃, under stirring fast, the water that adds 2-4 ℃ of temperature, be made into spinning slurry, the addition of water is decided by the viscosity of spinning slurry, and the falling ball viscosity of spinning slurry is 30-50 second.
The method of the spinning slurry deaeration described in the present invention is: allow spinning slurry under the vacuum condition of 650-700mmHg, leave standstill the air bubble of sloughing in 2-4 hour in the spinning slurry.
The described spinning of preparation regenerated cellulose viscose filament rayon is to use the wet-spinning frame spinning among the present invention, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 36-120 hole, the aperture is that the spinning head of 0.08-0.20mm is clamp-oned the coagulating bath coagulation forming, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter, coagulation bath temperature are 45-50 ℃, and draw ratio is 25-50%; Follow washing through 60-70 ℃; The alkali cleaning of the aqueous solution of the NaOH of 3-6 grams per liter; Again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter, after oiling, be wound into tube, drying the long filament of banana fiber cellulose fiber.
The described spinning of preparation regenerated fiber cellulose viscose short is to use the wet-spinning frame spinning among the present invention, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 400-1000 hole, the aperture is that the spinning head of 0.05-0.15mm is clamp-oned the coagulating bath coagulation forming, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter, coagulation bath temperature are 45-50 ℃, and draw ratio is 25-50%; Follow washing through 60-70 ℃; The alkali cleaning of the aqueous solution of the NaOH of 3-6 grams per liter; Again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter, oil, cut off, the staple fibre of dry banana fiber cellulose fiber.
Musaceae plant described in the present invention is bajiao banana and banana.
Particularly, the preparation method of regenerated cellulose viscose fiber of the present invention is: at first the cane to the Musaceae plant sorts, cuts off, with machinery knock, carding method divides silk, goes its leaf slag, colloid, rascal to obtain Musaceae fibre of plant element.With dilute alkaline soln the banana fiber element is come unstuck, slough residual colloid, after washing, drying, make Musaceae fibre of plant element.Handle Musaceae fibre of plant element with concentrated alkali solution then and make alkali cellulose, carry out yellow with carbon disulfide again and handle the solution that the alkali cellulose of making obtains cellulose xanthate, it is spinning slurry, extrude by spinnerets under acid bath with wet-spinning frame and to solidify, stretch, washing, last wet goods operation obtains described regenerated cellulose viscose fiber.
The invention has the beneficial effects as follows: with cane letter sorting, the cut-out of Musaceae plant; The stem stalk of Musaceae plant after cutting off is carried out machinery knock, adopt the method for combing to carry out the branch silk then, obtain the Musaceae string; Through this step, the contained lignin and the part of ash content are removed in the Musaceae plant haulm.Residual colloid removes with concentrated alkali solution in the Musaceae string that minute silk is obtained, and obtains the Musaceae plant cellulose again after washing drying; This step gets ready for the preparation alkali cellulose.Characteristics of the present invention are that described viscose is that the cane of Musaceae plant is that the cellulose that raw material extracts is produced, and the fiber of making can be an also long filament of staple fibre.This viscose has good flexibility, water imbibition, dyeability, can make separately fabric also can with other fiber blends, created new field for the exploitation of comprehensive utilization of Musaceae plant and tencel thereof thus.In the method for the invention, raw material sources are extensive, and, both efficiently solved banana planting ground environmental pollution problems to nowadays still carrying out twice laid as the cane of the Musaceae plant of refuse, can provide the regenerated cellulose viscose fiber that can take for society again.Owing to there not be the step of bleaching, so can also avoid a series of environmental problems of causing because of bleaching process.This technological process is short, equipment is simple, it is few to pollute, and can realize the production of cellulose viscose fibre industry.Prepared fiber product is comfortable and easy to wear, drapability good.
The specific embodiment
To help to understand the present invention by following examples, but not limit content of the present invention.
Embodiment 1
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 0.8% concentration expressed in percentage by weight boiled 3 hours, and liquor ratio is: 1:4; Washing, the dry banana fiber element that gets.
Plain to immerse temperature be 23 ℃ banana fiber again, and concentration is in the aqueous solution of NaOH of 250 grams per liters, flood after 110 minutes, takes out alkali cellulose, squeezes unnecessary alkali lye, and making and being with the weight percentage of alkali cellulose in the liquid caustic soda cellulose is 30%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 35% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 40 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 10 ℃, under stirring fast, the water that adds 4 ℃ of temperature is made into falling ball viscosity and is 30 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 650mmHg, leave standstill the air bubble of sloughing in 2.5 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 40 holes, the aperture is that the spinning head of 0.08mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 90 grams per liters, sodium sulphate 310 grams per liters, zinc sulfate 15 grams per liters, coagulation bath temperature is 45 ℃, and draw ratio is 45%; Follow washing through 60 ℃; Use the aqueous solution alkali cleaning of the NaOH of 3 grams per liters again; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, promptly get viscose filament yarn after oiling, be wound into tube, drying, resulting viscose filament yarn fineness is 2.4d tex, do strong for 2.2cN/dtex, wet be by force that 1.12cN/dtex, stem elongation rate are 16% faint yellow banana fiber cellulose fiber long filament.
Embodiment 2
With the bajiao banana cane with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.5% concentration expressed in percentage by weight boiled 1.8 hours, and liquor ratio is: 1:10; After washing, obtain the Basho fiber element.
Plain to immerse temperature be 18 ℃ Basho fiber again, and concentration is that liquor ratio is: 1:10 in the aqueous solution of NaOH of 240 grams per liters; Flood after 90 minutes, take out alkali cellulose, squeeze unnecessary alkali lye, making the weight percentage of alkali cellulose in the band liquid caustic soda cellulose is 33%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 25% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 60 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 14 ℃, under stirring fast, the water that adds 2 ℃ of temperature is made into falling ball viscosity and is 50 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 4 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 1000 holes, the aperture is that the spinning head of 0.10mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 120 grams per liters, sodium sulphate 290 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 50 ℃, and draw ratio is 40%; Follow washing through 70 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 6 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 3 grams per liters, oil, cut into the length of 36mm, drying obtains 2.2dtex, do strong for 2.6cN/dtex, wet strong be the plain staple fibre of Basho fiber of 18% faint yellow cotton type for 1.3cN/dtex, stem elongation rate.
Embodiment 3
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.0% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:5; Washing, the dry banana fiber element that gets.
Plain to immerse temperature be 20 ℃ banana fiber again, and concentration is in the aqueous solution of NaOH of 245 grams per liters, flood after 60 minutes, takes out alkali cellulose, squeezes unnecessary alkali lye, and making and being with the weight percentage of alkali cellulose in the liquid caustic soda cellulose is 31%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 28% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 50 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3.5 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 40mm, it is 2.7dtex that drying obtains line density, do strong for 2.8cN/dtex, wet strong be the regenerated cellulose viscose long fiber of 16% faint yellow wool type for 1.4cN/dtex, stem elongation rate.
Embodiment 4
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:6; Washing, the dry banana fiber element that gets.
Be the banana fiber element that to immerse temperature be 20 ℃ for the ratio of 1:3 in mass ratio again, concentration is in the aqueous solution of NaOH of 240 grams per liters, floods after 60 minutes, takes out alkali cellulose, squeeze unnecessary alkali lye, making the weight percentage of alkali cellulose in the band liquid caustic soda cellulose is 32%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 32% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 60 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 2 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 60 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 110 grams per liters, sodium sulphate 295 grams per liters, zinc sulfate 14 grams per liters, coagulation bath temperature are 48 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2.8 grams per liters, oil, cut into the length of 65mm, drying obtains 39dtex/40F, do strong for 2.4cN/dtex, wet strong be the plain long fiber of banana fiber of 18% faint yellow wool type for 1.2cN/dtex stem elongation rate.
Embodiment 5
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.2 hours, and liquor ratio is: 1:8; Washing, the dry banana fiber element that gets.
Be the banana fiber element that to immerse temperature be 20 ℃ for the ratio of 1:2 in mass ratio again, concentration is in the aqueous solution of NaOH of 240 grams per liters, floods after 110 minutes, takes out alkali cellulose, squeeze unnecessary alkali lye, making the weight percentage of alkali cellulose in the band liquid caustic soda cellulose is 33%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 28% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 50 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 40mm, drying obtains 2.7dtex, do strong for 2.9cN/dtex, wet strong be the banana regenerated cellulose viscose fiber of 18% faint yellow wool type for 1.45cN/dtex, stem elongation rate.
Embodiment 6
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:9; Washing, the dry banana fiber element that gets.
Be the banana fiber element that to immerse temperature be 20 ℃ for the ratio of 1:3 in mass ratio again, concentration is in the aqueous solution of NaOH of 240 grams per liters, floods after 60 minutes, takes out alkali cellulose, squeeze unnecessary alkali lye, making the weight percentage of alkali cellulose in the band liquid caustic soda cellulose is 31%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 33% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 45 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.13mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 36mm, drying obtains 2.5dtex, do strong for 2.3cN/dtex, wet strong be the banana fiber cellulose fiber of 16% faint yellow wool type for 1.15cN/dtex, stem elongation rate.
Embodiment 7
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:10; Washing, the dry banana fiber element that gets.
Plain to immerse temperature be 20 ℃ banana fiber again, and concentration is in the aqueous solution of NaOH of 240 grams per liters, flood after 60 minutes, takes out alkali cellulose, squeezes unnecessary alkali lye, and making and being with the weight percentage of alkali cellulose in the liquid caustic soda cellulose is 31%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 28% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 50 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 38mm, drying obtains 2.7dtex, do strong is the banana fiber cellulose fiber of 16% faint yellow wool type for 2.3cN/dtex, wet strong 1.15cN/dtex, stem elongation rate.
Embodiment 8
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:7; Washing, the dry banana stem stalk fiber element that gets.
Plain to immerse temperature be 20 ℃ banana stem stalk fiber again, and concentration is in the aqueous solution of NaOH of 240 grams per liters, flood after 60 minutes, takes out alkali cellulose, squeezes unnecessary alkali lye, and making and being with the weight percentage of alkali cellulose in the liquid caustic soda cellulose is 31%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 28% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 50 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 36mm, drying obtains 2.5dtex, do strong for 2.6cN/dtex, to do strong be the banana fiber cellulose fiber of 17% faint yellow wool type for 1.3cN/dtex, stem elongation rate.
Embodiment 9
The banana stalk of choosing, cut-out, with machinery knock, carding method, remove its leaf slag, colloid, rascal and obtain fiber; The fiber that divides silk to obtain, the sodium hydroxide solution of putting into 1.2% concentration expressed in percentage by weight boiled 2.5 hours, and liquor ratio is: 1:6; Washing, the dry banana fiber element that gets.
Be the banana fiber element that to immerse temperature be 20 ℃ for the ratio of 1:3 in mass ratio again, concentration is in the aqueous solution of NaOH of 240 grams per liters, floods after 60 minutes, takes out alkali cellulose, squeeze unnecessary alkali lye, making the weight percentage of alkali cellulose in the band liquid caustic soda cellulose is 31%.
The carbon disulfide of above-mentioned alkali cellulose that obtains and alkali cellulose weight 28% is reacted, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, 50 minutes reaction time, make cellulose xanthate, the cellulose xanthate that makes is cooled to 12 ℃, under stirring fast, the water that adds 3 ℃ of temperature is made into falling ball viscosity and is 38 seconds spinning slurry.
Allow above-mentioned spinning slurry under the vacuum condition of 700mmHg, leave standstill the air bubble of sloughing in 3 hours in the spinning slurry.
With nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through 400 holes, the aperture is that the spinning head of 0.15mm is clamp-oned the coagulating bath coagulation forming, the coagulating bath composition is the aqueous solution of following substances, and the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 100 grams per liters, sodium sulphate 300 grams per liters, zinc sulfate 13 grams per liters, coagulation bath temperature are 47 ℃, and draw ratio is 50%; Follow washing through 65 ℃; Again through the aqueous solution alkali cleaning of the NaOH of 4.5 grams per liters; Again through the pickling of the aqueous hydrochloric acid solution of 2 grams per liters, oil, cut into the length of 36mm, drying obtains 2.7dtex, do strong for 2.5cN/dtex, wet strong be the banana fiber cellulose fiber of 18% faint yellow wool type for 1.25cN/dtex, stem elongation rate.
Claims (16)
1. a regenerated cellulose viscose fiber comprises viscose filament yarn and viscose staple fibre, it is characterized in that described viscose filament yarn and viscose staple fibre all are that stem stalk with the Musaceae plant is that feedstock production obtains; The fineness of described viscose filament yarn and viscose staple fibre is 2.2-2.7dtex, and dried fracture strength is 2.3-2.9CN/dtex, and wet breaking strength is 〉=1.10CN/dtex that dried elongation at break is 〉=16%; The preparation method of described regenerated cellulose viscose fiber may further comprise the steps:
(1) the stem stalk of Musaceae plant is carried out machinery and knock, carry out the branch silk then, obtain the Musaceae string;
(2) will divide the colloid in the Musaceae string that obtains to remove with dilute alkaline soln, after washing, obtain the Musaceae plant cellulose again; Concrete grammar is: a fiber that divides silk to obtain, the dilute alkaline soln of putting into the NaOH that contains and be the percentage by weight 0.8-1.5% of over dry raw material boiled 2-3 hour, and liquor ratio is 1: 4-1: 10, after washing, drying the Musaceae plant cellulose;
(3) resulting Musaceae plant cellulose is mixed with concentrated alkali solution produce alkali cellulose, described concentrated base is that concentration is the aqueous solution of the NaOH of 240-250 grams per liter;
(4) alkali cellulose with gained carries out yellow after acid treatment, then its dissolving is made spinning slurry;
(5) spinning slurry with gained carries out spinning, obtains viscose.
2. regenerated cellulose viscose fiber according to claim 1 is characterized in that described step (1) carries out the process that machinery also comprises that the cane with the Musaceae plant sorts, cuts off before knocking to the cane of Musaceae plant.
3. regenerated cellulose viscose fiber according to claim 1, it is characterized in that in the described step (3) resulting Musaceae plant cellulose being mixed the concrete grammar of producing alkali cellulose with concentrated alkali solution is: it is 19-23 ℃ that the Musaceae plant cellulose is immersed temperature, concentration is in the aqueous solution of NaOH of 240-250 grams per liter, dipping is after 60-120 minute in this solution, take out alkali cellulose, after squeezing unnecessary alkali lye, the weight percentage of alkali cellulose is 30-33% in the band liquid caustic soda cellulose.
4. regenerated cellulose viscose fiber according to claim 1, the method that it is characterized in that alkali cellulose yellow in the described step (4), prepares spinning slurry is: with alkali cellulose and weight is that the carbon disulfide of alkali cellulose 25-35% reacts, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, reaction time 40-70 minute, make cellulose xanthate, then the cellulose xanthate that makes is cooled to 10-14 ℃, under stirring fast, add the water of 2-4 ℃ of temperature, make that the falling ball viscosity of spinning slurry is 30-50 second.
5. regenerated cellulose viscose fiber according to claim 1 is characterized in that also comprising the process of spinning slurry being carried out deaeration in the described step (5).
6. regenerated cellulose viscose fiber according to claim 5 is characterized in that the method for described spinning slurry deaeration is: allow spinning slurry under the vacuum condition of 650-700mmHg, leave standstill the air bubble of sloughing in 2-4 hour in the spinning slurry.
7. regenerated cellulose viscose fiber according to claim 1, it is characterized in that described spinning is to be spun into long filament with wet-spinning frame when the preparation regenerated cellulose viscose filament rayon, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 36-120 hole, the aperture is that the spinning head of 0.08-0.20mm is clamp-oned the coagulating bath coagulation forming, wherein the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter, coagulation bath temperature is 45-50 ℃, and draw ratio is 25-50%; Follow washing through 60-70 ℃; The alkali cleaning of the aqueous solution of the NaOH of 3-6 grams per liter; Again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter, after oiling, be wound into tube, drying regenerated cellulose viscose filament rayon; Described spinning is to be spun into staple fibre with wet-spinning frame when preparation regenerated fiber cellulose viscose short, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 400-1000 hole, the aperture is that the spinning head of 0.05-0.15mm is clamp-oned the coagulating bath coagulation forming, wherein the composition of coagulating bath is: sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter; Coagulation bath temperature is 45-50 ℃; Draw ratio is 25-50%; Then with temperature 60-70 ℃ wash, the aqueous solution of NaOH that concentration is the 3-6 grams per liter carries out alkali cleaning, again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter; Oil at last, cut off, the dry regenerated fiber cellulose viscose short that gets.
8. according to each described regenerated cellulose viscose fiber among the claim 1-7, it is characterized in that described Musaceae plant is bajiao banana or banana.。
9. method for preparing regenerated cellulose viscose fiber described in claim 1 is characterized in that described preparation method may further comprise the steps:
(1) the stem stalk of Musaceae plant is carried out machinery and knock, carry out the branch silk then, obtain the Musaceae string;
(2) will divide the colloid in the Musaceae string that obtains to remove with dilute alkaline soln, after washing, obtain the Musaceae plant cellulose again; Concrete grammar is: a fiber that divides silk to obtain, the dilute alkaline soln of putting into the NaOH that contains and be the percentage by weight 0.8-1.5% of over dry raw material boiled 2-3 hour, and liquor ratio is 1: 4-1: 10, after washing, drying the Musaceae plant cellulose;
(3) resulting Musaceae plant cellulose is mixed with concentrated alkali solution produce alkali cellulose, described concentrated base is that concentration is the aqueous solution of the NaOH of 240-250 grams per liter;
(4) alkali cellulose with gained carries out yellow after acid treatment, then its dissolving is made spinning slurry;
(5) spinning slurry with gained carries out spinning, obtains viscose.
10. method according to claim 9 is characterized in that described step (1) carries out the process that machinery also comprises that the cane with the Musaceae plant sorts, cuts off before knocking to the cane of Musaceae plant.
11. method according to claim 9, it is characterized in that in the described step (3) resulting Musaceae plant cellulose being mixed the concrete grammar of producing alkali cellulose with concentrated alkali solution is: it is 19-23 ℃ that the Musaceae plant cellulose is immersed temperature, concentration is in the aqueous solution of NaOH of 240-250 grams per liter, dipping is after 60-120 minute in this solution, take out alkali cellulose, after squeezing unnecessary alkali lye, the weight percentage of alkali cellulose is 30-33% in the band liquid caustic soda cellulose.
12. method according to claim 9, the method that it is characterized in that alkali cellulose yellow in the described step (4), prepares spinning slurry is: with alkali cellulose and weight is that the carbon disulfide of alkali cellulose 25-35% reacts, the reaction initial temperature is 22 ℃, final temperature is 16 ℃, reaction time 40-70 minute, make cellulose xanthate, then the cellulose xanthate that makes is cooled to 10-14 ℃, under stirring fast, add the water of 2-4 ℃ of temperature, make that the falling ball viscosity of spinning slurry is 30-50 second.
13. method according to claim 9 is characterized in that also comprising the process of spinning slurry being carried out deaeration in the described step (5).
14. method according to claim 13 is characterized in that the method for described spinning slurry deaeration is: allow spinning slurry under the vacuum condition of 650-700mmHg, leave standstill the air bubble of sloughing in 2-4 hour in the spinning slurry.
15. method according to claim 9, it is characterized in that described spinning is to be spun into long filament with wet-spinning frame when the preparation regenerated cellulose viscose filament rayon, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 36-120 hole, the aperture is that the spinning head of 0.08-0.20mm is clamp-oned the coagulating bath coagulation forming, wherein the coagulating bath composition is the aqueous solution of following substances, sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter, coagulation bath temperature is 45-50 ℃, and draw ratio is 25-50%; Follow washing through 60-70 ℃; The alkali cleaning of the aqueous solution of the NaOH of 3-6 grams per liter; Again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter, after oiling, be wound into tube, drying regenerated cellulose viscose filament rayon; Described spinning is to be spun into staple fibre with wet-spinning frame when preparation regenerated fiber cellulose viscose short, concrete grammar is: with nitrogen spinning slurry is pressed into and enters measuring pump after filter filters, through the 400-1000 hole, the aperture is that the spinning head of 0.05-0.15mm is clamp-oned the coagulating bath coagulation forming, wherein the composition of coagulating bath is: sulfuric acid 90-120 grams per liter, sodium sulphate 290-310 grams per liter, zinc sulfate 13-15 grams per liter; Coagulation bath temperature is 45-50 ℃; Draw ratio is 25-50%; Then with temperature 60-70 ℃ wash, the aqueous solution of NaOH that concentration is the 3-6 grams per liter carries out alkali cleaning, again through the pickling of the aqueous hydrochloric acid solution of 2-3 grams per liter; Oil at last, cut off, the dry regenerated fiber cellulose viscose short that gets.
16., it is characterized in that described Musaceae plant is bajiao banana or banana according to each described method among the claim 9-15.
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| CN106894114A (en) * | 2017-04-18 | 2017-06-27 | 广东洪兴实业有限公司 | A kind of preparation technology of the high tenacity tencel fiber with clothes |
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| CN114808173A (en) * | 2022-03-22 | 2022-07-29 | 上海飒卓新材料科技有限公司 | Method for preparing green regenerated cellulose fibers by using vinasse as raw material |
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